ANALYTICAL CHEMISTRY OF MATERIALS

Degree course: 
Corso di Second cycle degree in CHEMISTRY
Academic year when starting the degree: 
2020/2021
Year: 
1
Academic year in which the course will be held: 
2020/2021
Course type: 
Compulsory subjects, characteristic of the class
Credits: 
6
Period: 
First Semester
Standard lectures hours: 
48
Detail of lecture’s hours: 
Lesson (48 hours)
Requirements: 

Basic analytical chemistry and instrumental; knowledge about the structure of matter at the atomic and molecular level; basic knowledge of spectroscopy.

Final Examination: 
Orale

Written test (2 hours) based on two questions:
1- Describe of a specific analytical technique, theoretical bases, applications.
2- Propose an alternative analytical approach for the solution of a real problem taken from scientific literature.

The two questions have the same weight for the final evaluation.
For the first question we will evaluate both absolute knowledge and scientific rigor in the presentation of the theoretical bases, and the ability to organize a logical discourse that makes us understand how such phenomena can be the basis for an instrumental analytical technique.
For the second question we will evaluate both the organizational capacity in proposing a rigorous analytical protocol and the originality of the proposal itself.

Assessment: 
Voto Finale

The course's main objective is to provide students with the information needed to plan and deal with the analysis of materials, from the point of view of the characterization and chemical composition. The presented case studies, the result of multidisciplinary approach of "problem solving," are examples of how to implement these findings in order to develop personal understanding and skills in solving real problems.
At the end of the course, the student will be able to understand the application possibilities of the various analysis techniques presented both for the qualitative characterization of the materials and for the quantitative aspects of the chemical analysis.
This understanding will allow the student to apply these techniques also to real cases, discussing the possible alternatives and complementarities between the information obtained from the techniques in order to propose a rigorous and complete analytical protocol, that is, able to define the characteristics of the material, according to the analytical question proposed.
The exercise part will allow the student to understand the diagnostic process that underlies the definition of an analytical protocol, as well as the case studies presented.

The course will offer an overview of the main analytical techniques used in the analysis and characterization of materials.

- Introduction (4h)
Interaction radiation / particle-matter.
Dualism of concept "beam in - beam out" and associated analytical techniques.
The emission of electrons; photoelectric effect.
X-rays emission.
Emissions of particle/ion

-Spectroscopic techniques
X-Ray Fluorescence Spectrometry:XRF and Total Reflection XRF; theoretical signs; lines K, L, M; tools to dispersion of WDX wavelength and energy of EDS. Micro-XRF, Imaging techniques, XANES/EXAFS basis. (10h)
Raman spectroscopy: theoretical outline and comparison with the IR spectroscopy. (2h)
Moessbauer spectroscopy: theoretical outline and applications. (4h)

Surface and microscopy techniques
surface definition.
XPS-ESCA
Brief introduction to the theoretical aspects X-ray photo-electronic Spectroscopy (XPS); Application of XPS in chemical problems: Electron Spectroscopy for Chemical Applications (ESCA); concept of "binding energy" and use in chemical analysis; Examples of analysis; geometric factors; electronic factors. (8h)
SEM-EDAX; TEM
Brief introduction to the theoretical aspects of the interaction electron-matter; definition of secondary electrons, back-scattered and Auger electrons; use of electron microscopy and practical problems; Instrumental description (SEM), generation of secondary and back-scattered electrons images; X-ray generation and spectrum recording(EDAX); X-ray "imaging" techniques(X-ray mapping); low vacuum techniques ( "low vacuum"); description of TEM. (6h)
SIMS-ISS
Brief introduction to "particles" techniques; Secondary Ion Mass Spectrometry; Ion Scattering Spectrometry. (2h)
STM, AFM
A theoretical outline on the effect Tunnel; principle of tunneling microscope operation (Scanning Tunneling Microscopy); Atomic force microscopy (AFM); applications. (2h)

Thermal Analytical Techniques
Basic concepts; thermo gravimetric analysis TGA; Instrumental description and calibration; differential thermal analysis (DTA) and differential scanning calorimetry (DSC); Instrumental description and calibration; application examples. (6h)

- Applications and Tutorials (4h)

- Introduction (4h)
Interaction radiation / particle-matter.
Dualism of concept "beam in - beam out" and associated analytical techniques.
The emission of electrons; photoelectric effect.
X-rays emission.
Emissions of particle/ion

-Spectroscopic techniques
X-Ray Fluorescence Spectrometry:XRF and Total Reflection XRF; theoretical signs; lines K, L, M; tools to dispersion of WDX wavelength and energy of EDS. Micro-XRF, Imaging techniques, XANES/EXAFS basis. (10h)
Raman spectroscopy: theoretical outline and comparison with the IR spectroscopy. (2h)
Moessbauer spectroscopy: theoretical outline and applications. (4h)

Surface and microscopy techniques
surface definition.
XPS-ESCA
Brief introduction to the theoretical aspects X-ray photo-electronic Spectroscopy (XPS); Application of XPS in chemical problems: Electron Spectroscopy for Chemical Applications (ESCA); concept of "binding energy" and use in chemical analysis; Examples of analysis; geometric factors; electronic factors. (8h)
SEM-EDAX; TEM
Brief introduction to the theoretical aspects of the interaction electron-matter; definition of secondary electrons, back-scattered and Auger electrons; use of electron microscopy and practical problems; Instrumental description (SEM), generation of secondary and back-scattered electrons images; X-ray generation and spectrum recording(EDAX); X-ray "imaging" techniques(X-ray mapping); low vacuum techniques ( "low vacuum"); description of TEM. (6h)
SIMS-ISS
Brief introduction to "particles" techniques; Secondary Ion Mass Spectrometry; Ion Scattering Spectrometry. (2h)
STM, AFM
A theoretical outline on the effect Tunnel; principle of tunneling microscope operation (Scanning Tunneling Microscopy); Atomic force microscopy (AFM); applications. (2h)

Thermal Analytical Techniques
Basic concepts; thermo gravimetric analysis TGA; Instrumental description and calibration; differential thermal analysis (DTA) and differential scanning calorimetry (DSC); Instrumental description and calibration; application examples. (6h)

- Applications and Tutorials (4h)

Slides: see-e-learning

Surface Analysis – The Principal Techniques
JOHN C. VICKERMAN, IAN S. GILMORE
©2009 John Wiley & Sons Ltd

Handbook of Analytical Techniques
edited by Helmut Giinzler and Alex Williams
WILEY-VCH Verlag GmbH

Frontal lessons (44h), supported by slides which include both the theoretical and the applicative part; all slides are present on e-learning, divided into theoretical lessons and supplementary material which includes the case studies presented during the course.
Practical exercises (4h), set on the idea of communicating how to create an analytical protocol for the analysis of a solid sample. The activity is carried out in small groups, in which the student is not an active part, but participates in the presence in the analysis itself, managing the data obtained independently.
Students will use bibliographic indications received during the course to carry out a research that allows the compilation of an ab initio protocol.
Using data obtained through real analysis, they will then propose a solution to the problem posed.

Student reception:
2nd floor studio, Cubo building, via Valleggio 9, Como
appointment by e-mail, andrea.pozzi@uninsubria.it

Professors